Chromatography of polyolefin polymers

a technology of polyolefin polymer and chromatography, which is applied in the field of liquid chromatography, can solve the problems of limited separation efficiency obtained by prior art methods, tref and crystaf cannot be used to analyze amorphous polyolefin polymers, and tref and crystaf require a relatively long analysis tim

Active Publication Date: 2011-06-23
THE DOW CHEM CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, neither TREF nor CRYSTAF can be used to analyze amorphous polyolefin polymers.
Furthermore, both TREF and CRYSTAF require a relatively long a

Method used

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  • Chromatography of polyolefin polymers
  • Chromatography of polyolefin polymers
  • Chromatography of polyolefin polymers

Examples

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example 1

[0023]of the thermal gradient interaction chromatography. A metallocene polymerized ethylene-octene copolymer product (EO-1) is chosen for fractionation. EO-1 has a melt index of 0.82 g / 10 minutes and a density of 0.885 g / cm3; the sample for use in TGIC is prepared by weighing approximately 32 mg of polymer into a 10 ml GC glass vial, which is capped and placed in Crystallization Elution Fractionation (CEF) (PolymerChar, Spain) auto sampler. The instrument adds o-dichlorobenzene (ODCB), containing 300 ppm butylated hydroxytoluene (BHT) as an oxidation inhibitor, to the vial, producing a solution that is approximately 4 mg / mL in polymer. The dissolution is done by the autosampler at 160° C. for 90 minutes. The CEF is equipped with an IR-4 detector operating at 150° C. The delay volume (the volume that the first polymer fraction has to travel before reaching the detector) is 1.5 ml.

[0024]The column is a 10 cm long HYPERCARB column, part number 35005-104646, and the mobile phase is ODC...

example 2

[0029]the thermal gradient interaction chromatography on polymerized ethylene-octene (EO) polymers and blends. EO-2 has a melt index of 1 g / 10 minutes and a density of 0.865 g / cm3. EO-3 has a melt index of 66 g / 10 minutes and a density of 0.882 g / cm3. Blend #1 is 50:50(wt / wt) solution blend of a high density homopolymer polyethylene at melt index of 1 g / 10 min and density of 0.953 g / cm3, and EO-3. Blend #2 is a 50:50(wt / wt) solution blend of isotactic polypropylene at MFR (ASTM D 1238 condition 2.16 kg / 230° C.) of 13 g / 10 minutes and NIST SRM linear polyethylene 1484a.

[0030]The dissolution time is 120 minutes. The polymer solutions are loaded onto the column at 100° C. The polymer solution is kept at 100° C. for 2 minutes, and then cooled down to 80° C. at 20° C. / min, and kept at 80° C. for 5 minutes for thermal equilibrium, Polymer solution is eluted from 80° C. to 165° C. at 4° C. / min at a flow rate of 0.5 ml / min. Other experimental conditions are the same as Example 1. The chroma...

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Abstract

A method for multi-dimensional chromatography of a polyolefin polymer, comprising introducing a solution of the polyolefin polymer into a liquid flowing through a first liquid chromatography stationary phase or a field flow fractionation device and subsequently flowing the solution through a second liquid chromatography stationary phase, the second liquid chromatography stationary phase comprising graphitic carbon, the polyolefin polymer emerging from the liquid chromatography stationary phase with a retention factor greater than zero.

Description

BACKGROUND OF THE INVENTION[0001]The disclosed invention is in the field of liquid chromatography. Liquid chromatography is used by the art to analyze polymers with regard to molecular size by Size Exclusion Chromatography (SEC) and with regard to chemical composition by High Performance Liquid Chromatography (HPLC). This disclosure relates to HPLC analysis of polymers with regard to chemical composition.[0002]Polyolefin polymers (such as polymers and copolymers comprising polymerized ethylene monomer and / or propylene monomer) have long been analyzed with regard to chemical composition distribution by temperature rising elution fractionation (TREF) and crystallization analysis fractionation (CRYSTAF). However, neither TREF nor CRYSTAF can be used to analyze amorphous polyolefin polymers. Furthermore, both TREF and CRYSTAF require a relatively long analysis time. Therefore, the art turned to HPLC in an attempt to reduce analysis time and to expand the scope of analysis to amorphous p...

Claims

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Application Information

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IPC IPC(8): C08F6/00
CPCB01D15/161B01D15/166B01D15/1878B01J20/24B01J2220/4825G01N2030/885G01N30/34G01N2030/3076
Inventor WINNIFORD, WILLIAM L.CONG, RONGJUANSTOKICH, JR., THEODORE M.PELL, RANDY J.MILLER, MATTHEW D.ROY, ABHISHEKVAN DAMME, FREDDYDEGROOT, ALEXANDER W.LYONS, JOHN W.MEUNIER, DAVID M.
Owner THE DOW CHEM CO
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